Nitric Acid → HCID 178433475、化合物

HRID 541419ノート

反応式

HRID 541419 の反応式
[OH:1][C:2]1[N:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[OH:1][C:2]1[N:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 178425908HCID 178425908、化合物

生成物 1

HCID 178433475HCID 178433475、化合物収率 87.2%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒2 回

反応条件

温度
90 °C

実験手順

To a solution of 2-hydroxy-6-methylnicotinic acid (14.0 g, 91.5 mmol, 1.00 equiv) in sulfuric acid (conc.) (140 mL) at 0° C. was added dropwise a solution of HNO3 (12.0 g, 190 mmol, 2.00 equiv) in sulfuric acid (conc.) (10 mL). The resulting mixture was then stirred for 2 h at 90° C., cooled to ambient temperature, and then quenched with 250 mL of ice water. The resulting solids were collected by filtration and dried in an oven under reduced pressure to yield 15.8 g (87%) of the title compound as a yellow solid.

後処理

  1. temperaturecooled to ambient temperature
  2. customquenched with 250 mL of ice water
  3. filtrationThe resulting solids were collected by filtration
  4. customdried in an oven under reduced pressure

出典と根拠

ORDレコード
ord-e5cf01cd3b4b4d03b11cb49e81b5cb2e
出典データセット
uspto-grants-2014_10
特許番号
US08871790B2

反応ノート

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